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Institute
- Institut für Chemie (2913) (remove)
Layered structures are ubiquitous in nature and industrial products, in which individual layers could have different mechanical/thermal properties and functions independently contributing to the performance of the whole layered structure for their relevant application. Tuning each layer affects the performance of the whole layered system.
Pores are utilized in various disciplines, where low density, but large surfaces are demanded. Besides, open and interconnected pores would act as a transferring channel for guest chemical molecules. The shape of pores influences compression behavior of the material. Moreover, introducing pores decreases the density and subsequently the mechanical strength. To maintain defined mechanical strength under various stress, porous structure can be reinforced by adding reinforcement agent such as fiber, filler or layered structure to bear the mechanical stress on demanded application.
In this context, this thesis aimed to generate new functions in bilayer systems by combining layers having different moduli and/or porosity, and to develop suitable processing techniques to access these structures.
Manufacturing processes of layered structures employ often organic solvents mostly causing environmental pollution. In this regard, the studied bilayer structures here were manufactured by processes free of organic solvents.
In this thesis, three bilayer systems were studied to answer the individual questions.
First, while various methods of introducing pores in melt-phase are reported for one-layer constructs with simple geometry, can such methods be applied to a bilayer structure, giving two porous layers?
This was addressed with Bilayer System 1. Two porous layers were obtained from melt-blending of two different polyurethanes (PU) and polyvinyl alcohol (PVA) in a co-continuous phase followed by sequential injection molding and leaching the PVA phase in deionized water. A porosity of 50 ± 5% with a high interconnectivity was obtained, in which the pore sizes in both layers ranged from 1 µm to 100 µm with an average of 22 µm in both layers. The obtained pores were tailored by applying an annealing treatment at relevant high temperatures of 110 °C and 130 °C, which allowed the porosity to be kept constant. The disadvantage of this system is that a maximum of 50% porosity could be reached and removal of leaching material in the weld line section of both layers is not guaranteed. Such a construct serves as a model for bilayer porous structure for determining structure-property relationships with respect to the pore size, porosity and mechanical properties of each layer. This fabrication method is also applicable to complex geometries by designing a relevant mold for injection molding.
Secondly, utilizing scCO2 foaming process at elevated temperature and pressure is considered as a green manufacturing process. Employing this method as a post-treatment can alter the history orientation of polymer chains created by previous fabrication methods. Can a bilayer structure be fabricated by a combination of sequential injection molding and scCO2 foaming process, in which a porous layer is supported by a compact layer?
Such a construct (Bilayer System 2) was generated by sequential injection molding of a PCL (Tm ≈ 58 °C) layer and a PLLA (Tg ≈ 58 °C) layer. Soaking this structure in the autoclave with scCO2 at T = 45 °C and P = 100 bar led to the selective foaming of PCL with a porosity of 80%, while the PLA layer was kept compact. The scCO2 autoclave led to the formation of a porous core and skin layer of the PCL, however, the degree of crystallinity of PLLA layer increased from 0 to 50% at the defined temperature and pressure. The microcellular structure of PCL as well as the degree of crystallinity of PLLA were controlled by increasing soaking time.
Thirdly, wrinkles on surfaces in micro/nano scale alter the properties, which are surface-related. Wrinkles are formed on a surface of a bilayer structure having a compliant substrate and a stiff thin film. However, the reported wrinkles were not reversible. Moreover, dynamic wrinkles in nano and micro scale have numerous examples in nature such as gecko foot hair offering reversible adhesion and an ability of lotus leaves for self-cleaning altering hydrophobicity of the surface. It was envisioned to imitate this biomimetic function on the bilayer structure, where self-assembly on/off patterns would be realized on the surface of this construct.
In summary, developing layered constructs having different properties/functions in the individual layer or exhibiting a new function as the consequence of layered structure can give novel insight for designing layered constructs in various disciplines such as packaging and transport industry, aerospace industry and health technology.
This habilitation thesis summarises the research work performed by the author during the last quindecennial period. The dissertation reflects his main research interests, which revolve around quantum dynamics of small-sized molecular systems, including their interactions with electromagnetic radiation or dissipative environments. This covers various dynamical processes that involve bound-bound, bound-free, and free-free molecular transitions. The latter encompass light-triggered rovibrational or rovibronic dynamics in bound molecules, molecular photodissociation induced by weak or strong laser fields, state-to-state reactive and/or inelastic molecular collisions, and phonon-driven vibrational relaxation of adsorbates at solid surfaces. Although the dissertation covers different topics of molecular reaction dynamics, most of these studies focus on nuclear quantum effects and their manifestations in experimental measures. The latter are assessed through comparison between quantum and classical predictions, and/or direct confrontation of theory and experiment. Most well known quantum concepts and effects will be encountered in this work. Yet, almost all these quantum notions find their roots in the central pillar of quantum theory, namely, the quantum superposition principle. Indeed, quantum coherence is the main source of most quantum effects, including interference, entanglement, and even tunneling. Thus, the common and predominant theme of all the investigations of this thesis is quantum coherence, and the survival or quenching of subsequent interference effects in various molecular processes. The lion's share of the dissertation is devoted to two associated quantum concepts, which are usually overlooked in computational molecular dynamics, viz. the Berry phase and identical nuclei symmetry. The importance of the latter in dynamical molecular processes and their direct fingerprints in experimental observables also rely very much on quantum coherence and entanglement. All these quantum phenomena are thoroughly discussed within the four main topics that form the core of this thesis. Each topic is described in a separate chapter, where it is briefly summarised and then illustrated with three peer-reviewed publications. The first topic deals with the relevance of quantum coherence/interference in molecular collisions, with a focus on the hydrogen-exchange reaction, H+H2 --> H2+H, and its isotopologues. For these collision processes, the significance of interference of probability amplitudes arises because of the existence of two main scattering pathways. The latter could be inelastic and reactive scattering, direct and time-delayed scattering, or two encircling reaction paths that loop in opposite senses around a conical intersection (CI) of the H3 molecular system. Our joint theoretical-experimental investigations of these processes reveal strong interference and geometric phase (GP) effects in state-to-state reaction probabilities and differential cross sections. However, these coherent effects completely cancel in integral cross sections and reaction rate constants, due to efficient dephasing of interference between the different scattering amplitudes. As byproducts of these studies, we highlight the discovery of two novel scattering mechanisms, which contradict conventional textbook pictures of molecular reaction dynamics. The second topic concerns the effect of the Berry phase on molecular photodynamics at conical intersections. To understand this effect, we developed a topological approach that separates the total molecular wavefunction of an unbound molecular system into two components, which wind in opposite senses around the conical intersection. This separation reveals that the only effect of the geometric phase is to change the sign of the relative phase of these two components. This in turn leads to a shift in the interference pattern of the molecular system---a phase shift that is reminiscient of the celebrated Aharonov-Bohm effect. This procedure is numerically illustrated with photodynamics at model standard CIs, as well as strong-field dissociation of diatomics at light-induced conical intersections (LICIs). Besides the fundamental aspect of these studies, their findings allow to interpret and predict the effect of the GP on the state-resolved or angle-resolved spectra of pump-probe experimental schemes, particularly the distributions of photofragments in molecular photodissociation experiments. The third topic pertains to the role of the indistinguishability of identical nuclei in molecular reaction dynamics, with an emphasis on dynamical localization in highly symmetric molecules. The main object of these studies is whether nuclear-spin statistics allow dynamical localization of the electronic, vibrational, or even rotational density on a specific molecular substructure or configuration rather than on another one which is identical (indistinguishable). Group-theoretic analysis of the symmetrized molecular wavefunctions of these systems shows that nuclear permutation symmetry engenders quantum entanglement between the eigenstates of the different molecular degrees of freedom. This subsequently leads to complete quenching of dynamical localization over indistinguishable molecular substructures---an observation that is in sharp contradiction with well known textbook views of iconic molecular processes. This is illustrated with various examples of quantum dynamics in symmetric double-well achiral molecules, such as the prototypical umbrella inversion motion of ammonia, electronic Kekulé dynamics in the benzene molecule, and coupled electron-nuclear dynamics in laser-induced indirect photodissociation of the dihydrogen molecular cation. The last part of the thesis is devoted to the development of approximate wavefunction approaches for phonon-induced vibrational relaxation of adsorbates (system) at surfaces (bath). Due to the so-called 'curse of dimensionality', these system-bath complexes cannot be handled with standard wavefunction methods. To alleviate the exponential scaling of the latter, we developed approximate yet quite accurate numerical schemes that have a polynomial scaling with respect to the bath dimensionality. The corresponding algorithms combine symmetry-based reductions of the full vibrational Hilbert space and iterative Krylov techniques. These approximate wavefunction approaches resemble the 'Bixon-Jortner model' and the more general 'quantum tier model'. This is illustrated with the decay of H-Si (D-Si) vibrations on a fully H(D)-covered silicon surface, which is modelled with a phonon-bath of more than two thousand oscillators. These approximate methods allow reliable estimation of the adsorbate vibrational lifetimes, and provide some insight into vibration-phonon couplings at solid surfaces. Although this topic is mainly computational, the developed wavefunction approaches permit to describe quantum entanglement between the system and bath states, and to embody some coherent effects in the time-evolution of the (sub-)system, which cannot be accounted for with the widely used 'reduced density matrix formalism'.
Maytenus disticha (Hook F.), belonging to the Celastraceae family, is an evergreen shrub, native of the central southern mountains of Chile. Previous studies demonstrated that the total extract of M. disticha (MD) has an acetylcholinesterase inhibitory activity along with growth regulatory and insecticidal activities. beta-Dihydroagarofurans sesquiterpenes are the most active components in the plant. However, its activity in cancer has not been analyzed yet. Here, we demonstrate that MD has a cytotoxic activity on breast (MCF-7), lung (PC9), and prostate (C4-2B) human cancer cells with an IC50 (mu g/mL) of 40, 4.7, and 5 mu g/mL, respectively, an increasing Bax/Bcl2 ratio, and inducing a mitochondrial membrane depolarization. The beta-dihydroagarofuran-type sesquiterpene (MD-6), dihydromyricetin (MD-9), and dihydromyricetin-3-O-beta-glucoside (MD-10) were isolated as the major compounds from MD extracts. From these compounds, only MD-6 showed cytotoxic activity on MCF-7, PC9, and C4-2B with an IC50 of 31.02, 17.58, and 42.19 mu M, respectively. Furthermore, the MD-6 increases cell ROS generation, and MD and MD-6 induce a mitochondrial superoxide generation and apoptosis on MCF-7, PC9, and C4-2B, which suggests that the cytotoxic effect of MD is mediated in part by the beta-dihydroagarofuran-type that induces apoptosis by a mitochondrial dysfunction.
Modular toolkit of multifunctional block copoly(2-oxazoline)s for the synthesis of nanoparticles
(2021)
Post-polymerization modification provides an elegant way to introduce chemical functionalities onto macromolecules to produce tailor-made materials with superior properties. This concept was adapted to well-defined block copolymers of the poly(2-oxazoline) family and demonstrated the large potential of these macromolecules as universal toolkit for numerous applications. Triblock copolymers with separated water-soluble, alkyne- and alkene-containing segments were synthesized and orthogonally modified with various low-molecular weight functional molecules by copper(I)-catalyzed azide-alkyne cycloaddition (CuAAC) and thiol-ene (TE) click reactions, respectively. Representative toolkit polymers were used for the synthesis of gold, iron oxide and silica nanoparticles.
Efficient and low-cost anode materials for the sodium-ion battery are highly desired to enable more economic energy storage. Effects on an ultrathin carbon nitride film deposited on a copper metal electrode are presented. The combination of effects show an unusually high capacity to store sodium metal. The g-C3N4 film is as thin as 10 nm and can be fabricated by an efficient, facile, and general chemical-vapor deposition method. A high reversible capacity of formally up to 51 Ah g(-1) indicates that the Na is not only stored in the carbon nitride as such, but that carbon nitride activates also the metal for reversible Na-deposition, while forming at the same time an solid electrolyte interface layer avoiding direct contact of the metallic phase with the liquid electrolyte.
The response of the hydrogen molecular ion, H-2(+), to few-cycle laser pulses of different intensities is simulated. To treat the coupled electron-nuclear motion, we use adiabatic potentials computed with Gaussian-type basis sets together with a heuristic ionization model for the electron and a grid representation for the nuclei. Using this mixed-basis approach, the time-dependent Schrodinger equation is solved, either within the Born-Oppenheimer approximation or with nonadiabatic couplings included. The dipole response spectra are compared to all-grid-based solutions for the three-body problem, which we take as a reference to benchmark the Gaussian-type basis set approaches. Also, calculations employing the fixed-nuclei approximation are performed, to quantify effects due to nuclear motion. For low intensities and small ionization probabilities, we get excellent agreement of the dynamics using Gaussian-type basis sets with the all-grid solutions. Our investigations suggest that high harmonic generation (HHG) and high-frequency response, in general, can be reliably modeled using Gaussian-type basis sets for the electrons for not too high harmonics. Further, nuclear motion destroys electronic coherences in the response spectra even on the time scale of about 30 fs and affects HHG intensities, which reflect the electron dynamics occurring on the attosecond time scale. For the present system, non-Born-Oppenheimer effects are small. The Gaussian-based, nonadiabatically coupled, time-dependent multisurface approach to treat quantum electron-nuclear motion beyond the non-Born-Oppenheimer approximation can be easily extended to approximate wavefunction methods, such as time-dependent configuration interaction singles (TD-CIS), for systems where no benchmarks are available.
Poly(N,N-bis(2-methoxyethyl)acrylamide) (PbMOEAm) featuring two classical chemical motifs from non-ionic water-soluble polymers, namely, the amide and ethyleneglycolether moieties, was synthesized by reversible addition fragmentation transfer (RAFT) polymerization. This tertiary polyacrylamide is thermoresponsive exhibiting a lower critical solution temperature (LCST)-type phase transition. A series of homo- and block copolymers with varying molar masses but low dispersities and different end groups were prepared. Their thermoresponsive behavior in aqueous solution was analyzed via turbidimetry and dynamic light scattering (DLS). The cloud points (CP) increased with increasing molar masses, converging to 46 degrees C for 1 wt% solutions. This rise is attributed to the polymers' hydrophobic end groups incorporated via the RAFT agents. When a surfactant-like strongly hydrophobic end group was attached using a functional RAFT agent, CP was lowered to 42 degrees C, i.e., closer to human body temperature. Also, the effect of added salts, in particular, the role of the Hofmeister series, on the phase transition of PbMOEAm was investigated, exemplified for the kosmotropic fluoride, intermediate chloride, and chaotropic thiocyanate anions. A pronounced shift of the cloud point of about 10 degrees C to lower or higher temperatures was observed for 0.2 M fluoride and thiocyanate, respectively. When PbMOEAm was attached to a long hydrophilic block of poly(N,N-dimethylacrylamide) (PDMAm), the cloud points of these block copolymers were strongly shifted towards higher temperatures. While no phase transition was observed for PDMAm-b-pbMOEAm with short thermoresponsive blocks, block copolymers with about equally sized PbMOEAm and PDMAm blocks underwent the coil-to-globule transition around 60 degrees C.
A directed attractive interaction between predefined "patchy" sites on the surfaces of anisotropic microcolloids can provide them with the ability to self-assemble in a controlled manner to build target structures of increased complexity. An important step toward the controlled formation of a desired superstructure is to identify reversible electrostatic interactions between patches which allow them to align with one another. The formation of bipatchy particles with two oppositely charged patches fabricated using sandwich microcontact printing is reported. These particles spontaneously self-aggregate in solution, where a diversity of short and long chains of bipatchy particles with different shapes, such as branched, bent, and linear, are formed. Calculations show that chain formation is driven by a combination of attractive electrostatic interactions between oppositely charged patches and the charge-induced polarization of interacting particles.
Shape-memory polymers designed in view of thermomechanical energy storage and conversion systems
(2021)
Light-mediated polymerization techniques offer distinct advantages over polymerization reactions fueled by thermal energy, such as high spatial and temporal control as well as the possibility to work under mild reaction conditions. Reversible addition-fragmentation chain-transfer (RAFT) polymerization is a highly versatile radical polymerization method that can be utilized to control a variety of monomers and produce a vast number of complex macromolecular structures. The use of light to drive a RAFT-polymerization is possible via multiple routes. Besides the use of photo-initiators, or photo-catalysts, the direct activation of the chain transfer agent controlling the RAFT process in a photo-iniferter (PI) process is an elegant way to initiate and control polymerization reactions. Within this review, PI-RAFT polymerization and its advantages over the conventional RAFT process are discussed in detail.